电感耦合等离子体原子发射光谱法测定锑锭中9种微量元素  

Determination of 9 micro elements in antimony ingot by inductively coupled plasma atomic emission spectrometry

作　　者：卞大勇 刘淑香 姚旭 BIAN Dayong;LIU Shuxiang;YAO Xu(Tianjin Huakan Commodity Inspection Co.,Ltd.,Tianjin 300181,China)

机构地区：[1]天津华勘商品检验有限公司,天津300181

出　　处：《冶金分析》2024年第3期65-71,共7页Metallurgical Analysis

摘　　要：锑锭中的微量元素含量是确定锑锭品质的主要指标,现行国家标准方法(GB/T 3253.X—2008/2009)操作难度大、效率低,开发新方法极具现实意义。使用王水在低温下溶解样品,并使用氢氟酸抑制锑的水解,选择Pb 220.353 nm、Fe 259.940 nm、Cu 324.754 nm、Cd 214.438 nm、As 193.759 nm、Se 196.090 nm、Bi 190.234 nm、Hg 194.227 nm、S 180.731 nm为Pb、Fe、Cu、Cd、As、Se、Bi、Hg、S的分析谱线,以基体匹配法绘制校准曲线消除基体效应的影响,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定锑锭中Pb、Fe、Cu、Cd、As、Se、Bi、Hg、S等9种微量元素的方法。各元素的校准曲线线性相关系数r均大于0.9995,方法检出限为0.000020%~0.00021%,定量限为0.000067%~0.00070%。按照实验方法测定锑锭样品中9种微量元素,结果的相对标准偏差(RSD,n=10)为1.3%~9.4%,与国家标准方法(GB/T 3253.X—2008/2009)比对结果相一致。The contents of micro elements in antimony ingot are main indexes to determine its quality.The current national standard method(GB/T 3253.X-2008/2009)has some shortcomings such as high operation difficulty and low efficiency,so it is of great significance to develop new determination method.In this paper,the sample was dissolved with aqua regia at low temperature.The hydrolysis of antimony was inhibited by adding hydrofluoric acid.Pb 220.353 nm,Fe 259.940 nm,Cu 324.754 nm,Cd 214.438 nm,As 193.759 nm,Se 196.090 nm,Bi 190.234 nm,Hg 194.227 nm and S 180.731 nm were selected as the analytical lines for Pb,Fe,Cu,Cd,As,Se,Bi,Hg and S,respectively.The influence of matrix effect was eliminated by drawing calibration curves with matrix matching method.Thus,a method for determination of 9 micro elements(Pb,Fe,Cu,Cd,As,Se,Bi,Hg and S)in antimony ingot was established by inductively coupled plasma emission spectrometry(ICP-AES).The linear correlation coefficients(r)of calibration curves of elements were greater than 0.9995.The limits of detection of this method were 0.000020%-0.00021%,and the limits of quantification were 0.000067%-0.00070%.9 micro elements in antimony ingot samples were determined according to the proposed method.The results were consistent with those obtained by national standard method(GB/T 3253.X-2008/2009),and the relative standard deviations(RSD,n=10)of determination results were between 1.3%and 9.4%.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 锑锭 微量元素 

分 类 号：O657.31[理学—分析化学] TG115.31[理学—化学]